微乳液相色谱法测定南、北五味子中5种木脂素类成分  

Simultaneous Determination of Five Major Lignans from Schisandrae Sphenantherae Fructus and Schisandrae Chinensis Fructus by Microemulsion Liquid Chromatography

作　　者：薛晖[1] 王新[1] 葛新[1] 

机构地区：[1]山西医科大学药学院,山西太原030001

出　　处：《中国中医药信息杂志》2015年第5期94-98,共5页Chinese Journal of Information on Traditional Chinese Medicine

摘　　要：目的：建立一种稳定、灵敏的o/w型微乳液相色谱法,同时测定南、北五味子中五味子醇甲、五味子醇乙、五味子酯甲、五味子甲素、五味子乙素5种木脂素类成分。方法采用Kromasil C18色谱柱（250 mmx4.6 mm,5μm）,通过考察微乳系统的组成对分离效果及保留时间的影响,以最优微乳体系[3.3%十二烷基磺酸钠（SDS,W/V）,1.2%正辛醇（V/V）及6.6%正丁醇（V/V）]-20 mmol/L磷酸盐（用磷酸及氢氧化钠调节pH 7.0）为流动相,流速0.7 mL/min,检测波长254 nm,柱温25℃。结果在优化条件下,5种木脂素类成分在20 min内达到基线分离,分离良好。五味子醇甲、五味子醇乙、五味子酯甲、五味子甲素、五味子乙素分别在2.0-155.0、8.3-166.7、8.8-175.8、8.3-166.7、8.9-177.1μg/mL范围内线性关系良好（r＞0.999）。检测限为0.06-0.18μg/mL,定量限为0.17-0.55μg/mL,平均加样回收率为97.22%-100.8%。结论所建立的方法准确、简单易行,可用于不同产地的南、北五味子中5种木脂素类成分的含量测定。Objective To develop a stable and sensitive microemulsion liquid chromatography method by using oil-in-water microemulsion mobile phase;To simultaneously determine five major active lignans, namely, schizandrin, schisandrol B, schisantherin A, deoxyschizandrin, and schisandrin B, in Schisandrae Sphenantherae Fructus and Schisandrae Chinensis Fructus. Methods The quantitative determination was conducted by using Kromasil C18 column （250 mmx 4.6 mm, 5μm）. The influence of the composition of the microemulsion system on separation effect and retention time was studied. The method was optimized to sodium dodecyl sulfonate 3.3%（SDS, W/V）, n-octanol 1.2% （V/V） and n-butanol 6.6% （V/V） in 20 mmol/L phosphate buffer （adjusted to pH 7.0 with orthophosphoric acid and sodium hydroxide）. The flow rate was set at 0.7 mL/min. The compound peaks were detected by UV at 254 nm. The column temperature was 25 ℃. Results Under the optimized conditions, baseline separation of 5 lignans was achieved in 20 min, and the separation was satisfying. Schizandrin, schisandrol B, schisantherin A, deoxyschizandrin, and schisandrin B were in linear relation within the ranges of 2.0-155.0, 8.3-166.7, 8.8-175.8, 8.3-166.7, 8.9-177.1μg/mL （r〈0.999）. The limit of detection ranged from 0.06μg/mL to 0.18μg/mL, and the limit of quantitation ranged from 0.17μg/mL to 0.55μg/mL. The average recovery values were between 97.22%and 100.8%. Conclusion This method is simple, accurate and reliable, and can be successfully applied to simultaneous determination of five major active lignans in 13 batches of Schisandrae Sphenantherae Fructus and Schisandrae Chinensis Fructus from different producing areas in China.

关 键 词：微乳液相色谱 南五味子 北五味子 木脂素 

分 类 号：R284.1[医药卫生—中药学]